Inorganic thermoplastic composition



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' I monemc THERMOPLASTIC -COM- POSITION I Willis A, Boughton, Cambridge, Mass., assignor to New England Mica 00., corporation of Massach Application January 10, 1931, Serial No. 507,991

v "No Drawing.

This invention relates to inorganic thermoplastic compositions, which soften and become sufliciently plastic by the application of relatively v --moderate heat, for example, up to about 400 C.

to be suitably manipulated or shaped, and which are resistant to practically all organic liquids; solvents, and compounds, and which when solid, are fairly resistant to water and non-corrosive Y aqueous solutions.

L 4 1 -An object of the invention is to provide an in organic reversibly thermoplastic composition which may be used as a luting or joining or sealing composition between a variety of substances,

' --for example, metal pipe glass pipe joints, terra cotta pipe joints, joints between dissimilar substances: etc., which ,are in contact with or convey organic liguids or similar products in commercial chemical manufacturing operations, also for certain types of linings, and for analo gous uses.

A further object is to provide an inorganic reversibly thermoplastic composition which upon controlled heating will become sufliciently soft and plastic to form a seal and to firmly unite with other materials to form a perfect bond therewith, and which on cooling will stiffen and become highly viscous, or semi-solid, or solid, whereby fractures in chemical apparatus, etc., may be repaired, or several parts may be united into a unitary leak-proof apparatus, or covers luted to vessels, etc, j

'A further object is to provide aseries of inorganic reversibly thermoplastic compositions which may be used as efiective seals or lutes at 5 particular temperatures; the composition becoming progressively fluid at increasing temperatures, and progressively viscous masses at decreasing temperatures until they are semisolid to solid, thereby providing a great variety 40 of compositions which function as seals under a great variety of operating conditions.

Other objects of the invention will be apparent to those skilled in the art upon reading the specification.

In thev preparation of these inorganic thermoplastic composition, I have taken advantage of the property peculiar to only a very few inorganic substances of forming aqueous solutions which when heated under properly regulated coni 60 ditions do not precipitatethe dissolved salt, but

glass-like solids or"super-'cool'ed fluids may be I! about 80 C.

Waltham, Mass, a usetts described as being colloidally associated with the substance.

Examples of these few substances are the water soluble .metal. grtahoshates metaborates now e er own as monoorates, F

for example, the potassium and sodium com- P u d metaphgsphcgic acid, and alkali metal silicates. While such substances do ac a 1 e m an emperature ranges of dehydration and viscosity, they have the same general properties herein described. For example, a dilute water solution of sodium metaphosphat'e'-'isa"'mobile ifluid at ordinary temperatures, much like that of any water soluble inorganic salt. But when this solution is concentrated under properly controlled conditions it remains a comparative mobile fluid up to temperatures well above 250 C. and at this temperature still contains approximately five percentoiwater; and when then cooled to about 150 C., it is so viscous that ather mometer may be rotated in the mass onlywith difficulty. a ,I. The cooled product is semi-solidto-solid -according to the water content, and in the absence of a more appropriate term to define its physical properties, it may be regarded as a more-or-less solid solution of the ,dissolved substance in water. Similarly, a water solution of metaphosphoric acid when heated to boiling, boils continuously while the temperature rises gradually, and at a "regular rate, above 100 C., losing the'more tightly held water of association as the temperature rises. At 350 C. it still boils as a comparatively mobile fluid, although it contains only approximately five percent of water orless," and this mixture when cooled to 120 C. is so viscous that a thermometer may be rotated in the mass only withdifliculty. I a

7 Commercial sodium silicate solution (water glass), for example, is viscous even at ordinary.

' temperatures and cannot be used for the purposes described herein at temperatures above about 80 C. because of the intumescence that takes place 'due to the solidification. Consequently, thermoplastics covered by this invention, involving the use of sodium silicate solution must be used below as statedabovasubstances of the Therefore,

class described herein, and coming within the scope of this invention, give solutions having dif-' ferent ranges of temperature of dehydration and viscosity," but all can be treated so as toiexhibit the peculiar property of not precipitating as they dehydrate, abut yield solutions not increasing viscosity at lower temperatures. E:-l.-.

i i L 106. comPos'mous,

COATING R PLASTIC.

In general these specially prepared cooled fluids Uross iiiiliifcnw proximately twenty-one grams of finely powdered act like organic thermoplastic solids, inthat when mica. The application of heat is con mue unthey are again heated to the higher temperatures til the temperature is re they again become fluid, just like asphalt. That I is, the change from the fluid state to the solid state through a great range of viscosity is reversible, 9. property that is anomalous in the chemistry of simple inorganic substances. W m

These special solutions of high viscosity and low 10 water content may under certain limited condi-- tions themselves be used as reversible inorganic thermoplastics, but I prefer to mix with them various proportions of non-reacting finely powdered solid inorganic substances,- such as kaolin, graphite, mica, talc, etc., to give greater substance to the mass and provide a body that is more'ea'sily worked and handled. Examples of compositions are given hereafter, but each composition will vary in percentage according to the particular use desired. For some purposes, a porous fabric such .as burlap, may be saturated or coated with layers of the hot fluid and applied to a joint to be luted; vor a layer of fluid may be applied to the joint, then a layer of saturated or unsaturated fabric, Q5 and if desired, a flnal coating of fluilL I In practice I make an aqueous solution of the inorganic water-soluble substance of the class herein described containing roughly from twenty percent to forty percent of solid substance, or I [Q ,may take a solution containing two or more of such solid substances, and add thereto the desired .amount of a finely divided non-reacting inorganic solid in the proportion by weight of about 2 to 4 parts to about 7 parts of the dissolved substance a; pm a dry basis. This mixture is then stirred and heated until the temperature has reached the desired point when the mass is cooled and shaped into convenient forms while cooling. Such a mix- ;ture is a plastic fluid, capable of inelastic deforlo nation under stress, a viscous paste of putty- 1like or molasses-like consistency at the temperature at which it is to be used and is increasingly .viscous as the temperature is lowered, for example like asphalt, and may be described as be- 1,5 ring relatively low-temperature-softening, viscous, stifi, asphalt-like in character becoming a highly viscous non-flowing stiff, deformation resisting solid at temperatures C. to 200 C. below the liquid or putty-like point. v I a I find it desirable, furthermore, to vary the .percentage of added non-reacting inorganic solid,

e w ch will produce a mass having the desired degree of plasticity at the temperature of use. The desired degree of plasticity will vary with the :particular use to which the product is tobe applied and temperature-of-application; at a temperature of 110 C. the mass will contain approximately y-six percent of water; at a temperature of 12 Q. the

will contqin; approximately twenty percent of water; at a temperature of 10 C. the mass will contain approximately 5.8 perce ater; and at atempcratu're of 200 C. the mass will contain approximately thr cent of water. A mass showing thermoplastic properties at any desired temperaturelower than or intermediate between any oi' these specified temperatures will be obtained by. stopping the application of excess of heat "at that temperature. The product objoined at atemperature of C. will be found very eflicient for one class of :work in that it will be sufficiently plastic for application at that temperature, but will be semi-solid at lower or ordinary temperatures,and will thus produce an ei- :i-100 tective seal orlute in many types of chemical apparatus. -The product obtained at C. will be found to be eflicient as a lute at temperatures above those at which the 110 C. product can be .used; the product obtained at150 C. will 'be 105 found to produce an efiective seal or lute at still .higher temperatures, etc. The products obtained at the several temperatures will be found to be efilcient for difierent classes of work in-many chemical processes in which organic solvents 015110 reagents are used, and which involve different temperatures and operations.

example 2.'Metdphosphoric acid comma-z Meta hos horic acid is obtained commerciallyusually in ie iorm of glassy sticks. "Approxi- 'mately thirty-five grams of this material are dissolved in-IOO to-200 cubic centimeters of water with the'application-m controlled'heat, an {the mixture is addedapproximately twenty gramsor'flnely dw e m Thismixture-is heated-and 'at con ems-approximately m ty two'perce'nt of water; at l25 C. appmxa mmytwenty- 1cmpercent of mt-450 ="cpp 1 ai 1y percentor water adm C. approximately three percent ot waterfl m- .ror-example, kaolin, depending on the temperature qacid is therefore. hdapwd .mridifierent :55 resulting mass will have the desired thermoplastic properties herein described and claimed.

Examples illustrating several methods of preparing reversible thermoplastic compositions in accordance with this invention are as follows- Tltxample 1.Sodium metdphosphate Thirty-five grams of water soluble sodium meta hos hate are dissolved in .from 100 to 205 cubic cenimeters of waterwiththe aid of controlled heat. With Wnutionas mixed a --ranges bi temperature A and diflerent' classes of work than is sodium "metaphosphate.-'- However, the general principles or manuIactui'eand-appli- 'cation arethe same as those previously cited.

lE-m mple mwtabofate I Y', sodiiim' metaborateis dissolved in water and me W). a e y wdered non-re 0 mg powder such as talci graphite etc., and heated. I iI'he composition 0 e so um metabora e sea 5 are made in substantially "thesame' "way as the sodium ,metaphosphate compositions; and F exhibit ,entirely'hnalogous" changes of properties, fuses, and conditions of use asexistwiththe sodium emba s esamnes a; s-

- .ssde eiisevemae 1w 0;. i-: a... r,, Quantitiesof "sodium tahoshate, and sodium tetrabora w c is I e erewi msibly thermopiasti ties ewhenwinrcombination with the vil'netaphosp hate, eareidissolved' inamater and to :the soliition are Exercise.

Wicular object to be accomp the same way as in the exam a hite. At 80 "pro'xim'hfily seventeen percent of water and is added powders, for example kaolin and wdered micainsuitable proportions w lished, and the mixed mass heated and treated in substantially les above described; the resulting product exhibits entirely analogous changes of properties, uses, and conditions or use as exist with the other compositions herein described.

Example 5.Silicate of soda composition Ordinary water glass containing about forty percent 0 so so ate is mixed with approximately twenty grams of finely powdered 0. this mixture contains apout 100 C. it 585 r g y, I mix um graphite is adapted to still other temperature ranges and conditions of use than the previous examples.

In using any of the thermoplastic compositions to seal or lute a joint in a pipe, the pipe surfaces are cleaned, and the suitably heated thermoplastic composition is applied with a trowel, for example as with mortar, or with a spatula, knife or other forming tool, coating the parts to be sealed, and upon cooling, the composition becomes a self-sustaining hly viscous body, eiiectively closing the joint. A similar procedure is followed when it is desired to seal a crack in a broken vessel.

All of the above described compositions are integral mixtures of a more-or-less solid solution of a soluble substance or substances in water of the class described which do not separate out on concentration, and a powdered inert non-soluble solid, and have the general property of being reversibly thermoplastic, and selected compositions may be used for special applications. All seals or joints made by these compositions may be opened upon the application of an excess oi heat, and thereafter may be again sealed or luted as described above by cooling. When in the solid state, the product may be suitably pulverized, or the product may be molded into sticks, bars, etc., and packed for shipment.

I claim:

1. A composition of matter consisting of from about three percent to about six percent of water associated with metaphosphoric acid, which does not crystallize or separate out on cooling from a hot solution, said composition also containing an inert filler, and having the property oi bein reversibly thermoplastic.

2. A composition of matter consisting oi from about three percent to about fifteen percent of water associated with metaphosphoric acid, which does not crystallize or separate out on cooling from a hot solution, said composition also containing an inert filler and having the property or being reversibly thermoplastic.

3..A composition of matter consisting of from about three percent to about six percent of water associated with sodium metaphosphate, which does not crystallize or separate out on cooling from a hot solution, said composition also containing an inert filler, and having the property of being reversibly thermoplastic.

4. A composition of matter consisting of from about three percent to about fifteen percent of water, associated with sodium metaphosphate, which does not crystallize or separate out on cooling from a hot solution, said composition also containing an inert filler, and having the property of being reversibly thermoplastic.

5. A composition of matter consisting of from about three percent to about ten percent of water, associated with a sodium metaborate which does not crystallize or separate out on cooling from a hot solution, said composition also containing an inert filler, and having the property of being reversibly thermoplastic.

6. A composition of matter containing about two parts by weight of a metaphosphate and about one part by weight of inert matter, said weights being on a dry basis, said composition containing from about three percent to about fifteen percent of water, said water being associated with said metaphosphate, said metaphosphate having the property of not crystallizing or separating out on cooling from a hot solution, said inert matter being intimately difiused through said water association of the metaphosphate, and said composition having the property of being reversibly thermoplastic.

'7. A composition of matter containing about two parts by weight of a metaborate and one part by weight of inert matter, said weights being on a dry basis, said composition containing from about three percent to about fifteen percent 01 water, said water being associated with said metaborate, said metaborate having 'the property of not crystallizing or separating out from a hot solution, said inert matter being intimately diffused through said water association of the metaborate, and said composition having the property of being reversibly thermoplastic.

8. An inorganic reversibly thermoplastic sealing composition, consisting of a solid solution of water and at least one of the group of metaphosphoric acid, alkali metal metaphosphates, and alkali metal metaborates, mixed with a powdered inert solid, the water present being sufficient to produce a reversibly thermoplastic mass.

9. An inorganic rever 'bly thermoplastic sealing composition, consisting of a solid solution of water and at least one of the group of metaphosphoric acid, alkali metal metaphosphates, and alkali metal metaborates, mixed with a powdered inert solid, the water being present in from about three percent to about thirty-six percent of the resulting composition.

10. An inorganic reversibly thermoplastic sealing composition, consisting of a solid solution of water and at least one of the group of metaphosphoric acid, alkali metal metaphosphates, and a blendable alkali metal borate, mixed with a powdered inert solid, the water present being sufiicient to produce a reversibly thermoplastic mass.

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